| 研究生: |
沈姿誼 Tzu-Yi Shen |
|---|---|
| 論文名稱: |
具硫基官能基之中孔洞材料 SBA-1 的合成與鑑定 Synthesis and Characterization of Cubic Mesoporous Silicas SBA-1 with Thiol Functionality |
| 指導教授: |
高憲明
Hsien-Ming Kao |
| 口試委員: | |
| 學位類別: |
碩士 Master |
| 系所名稱: |
理學院 - 化學學系 Department of Chemistry |
| 畢業學年度: | 94 |
| 語文別: | 中文 |
| 論文頁數: | 103 |
| 相關次數: | 點閱:4 下載:0 |
| 分享至: |
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中文摘要
在本篇研究是以MPTMS ((3-Mercaptopropyl)trimethoxysilane) 與TEOS (Tetraethtyl orthosilicate) 為共同矽源,使用 C16TEABr (cetyltriethylammonium bromide) 作為模板試劑,在反應溫度為273 K下直接合成具有硫基官能基的中孔洞材料SBA-1,之後經由HCl / EtOH溶劑做萃取處理,移除模板後,得到的中孔洞材料仍然具有SBA-1的結構存在。研究發現硫基官能基化的中孔洞材料SBA-1,其MPTMS含量可達20%,對於中孔洞立方結構不會造成相轉變或是結構破壞,而其表面積、孔洞體積以及孔洞直徑均會隨MPTMS含量的增加而有遞減的趨勢。
藉由改變不同的酸量、不同的水熱時間、不同的攪拌時間以及不同矽源,探討對於合成具有硫醇官能基的SBA-1的影響。在改變不同的酸量的方面,可以觀察到不同的結果,在XRD 的結果中,可發現隨著酸量的增加,可加入在SBA-1中的MPTMS 之含量也隨之增加,而在29Si MAS NMR也觀察到隨著酸量的增加,有助於中孔洞材料SBA-1結構的穩定。在水洗測試也可得知,加入官能基可以有效的改善SBA-1結構不能水洗及不能溶劑萃取的缺點。
Abstract
One-step synthesis of well-ordered cubic mesoporous silicas SBA-1 containing simultaneously tetraethoxysilane (TEOS) and 3-mercapto- propyltrimethoxysilane (MPTMS) and has been synthesized by cetyltriethylammonium bromide (CTEABr) under strongly acidic conditions. In order to get optimized the thiol-functionalized mesoporous silicas SBA-1 which has been studied by in a wide range of synthesis conditions. All kinds of results of formating the parameter, including the relative reagent concentration (TEOS/MPTMS ratio), HCl concentration, synthesis temperature, and hydrothermal time.
The materials obtained were characterized by a variety of techniques including powder X-ray diffraction (XRD), nitrogen sorption measurements, 13C and 29Si magic angle spinning (MAS), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA).
The lower TEOS/MPTMS ratios resulted in materials with higher functional group loadings. The direct synthesis of thiol- functionalized SBA-1 materials, the concentration of MPTMS that can co-condense with TEOS will be up to 20% without observing a significant loss in the structure order and uncontrollable phase transformation of the cubic SBA-1 mesostructure. The HCl concentration of change was found that can determine the stability of thiol-functionalized SBA-1 towards the solvent extraction treatment. The difference in the morphology between pure SBA-1 and thiol- functionalized SBA-1 becase of the incorporated MPTMS can slow down the condensation rate of TEOS.
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